EP0193829B1 - Dust free particulate enzyme formulation - Google Patents

Dust free particulate enzyme formulation Download PDF

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Publication number
EP0193829B1
EP0193829B1 EP86102374A EP86102374A EP0193829B1 EP 0193829 B1 EP0193829 B1 EP 0193829B1 EP 86102374 A EP86102374 A EP 86102374A EP 86102374 A EP86102374 A EP 86102374A EP 0193829 B1 EP0193829 B1 EP 0193829B1
Authority
EP
European Patent Office
Prior art keywords
enzyme
core material
particulate
coated
particles
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP86102374A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0193829A3 (en
EP0193829A2 (en
Inventor
Ivan C. Good
Yun C. Jao
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Danisco US Inc
Original Assignee
Haarmann and Reimer Corp
Solvay Enzymes Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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Application filed by Haarmann and Reimer Corp, Solvay Enzymes Inc filed Critical Haarmann and Reimer Corp
Publication of EP0193829A2 publication Critical patent/EP0193829A2/en
Publication of EP0193829A3 publication Critical patent/EP0193829A3/en
Application granted granted Critical
Publication of EP0193829B1 publication Critical patent/EP0193829B1/en
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
    • C11D3/38672—Granulated or coated enzymes
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N9/00—Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
    • C12N9/98—Preparation of granular or free-flowing enzyme compositions

Definitions

  • This invention relates to a procedure for making dry and dust free enzyme granules particularly useful for use with laundry detergents.
  • the manufacture of enzymatic washing and cleaning agents by incorporating powdered, highly active enzyme concentrates by mixing them with common cleaning agents is well known.
  • the washing agents manufactured in this manner tend to form enzyme dusts which can cause dermatologic damage both to the manufacturer and the consumer of the enzyme powder containing washing composition.
  • German AS 21 37 042 discloses a process in which an extrudable enzyme containing formulation is extruded through a die onto the revolving plate of a spheronizing device to form spherical particles of the enzyme containing formulations which are optionally coated with a material designed to prevent dusting.
  • U.S. Patent No. 4,016,040 discloses a method for the preparation of free-flowing substantially dust free, spherical enzyme containing beads prepared by blending a powdered concentrate of the enzyme with a binder in molten form and spraying droplets of the blend through a spray nozzle into cool air to solidify the droplets and form the beads.
  • U.S. Patent No. 4,009,076 Another type of granular enzyme formulation is described in U.S. Patent No. 4,009,076.
  • This formulation is prepared by mixing the dry enzyme with a solid non-viable substance and optionally a cohesive organic material as binder to form an enzymatically active core.
  • An enzyme slurry containing the cohesive organic material can be sprayed onto, for example, sodium tripolyphosphate in a mixer or an enzyme powder can be mixed with the sodium tripolyphosphate and the cohesive organic material sprayed onto it with subsequent extrusion through a die.
  • the enzyme containing granule is sprayed with an aqueous solution containing a plasticized organic resin and then dried.
  • a process is described in DDR Patent No. 0 151 598 in which sodium tripolyphosphate is sprayed with an aqueous enzyme solution and agglomerated in a cyclone apparatus.
  • the agglomerates are removed from the cyclone apparatus while still wet and placed in a mechanical blender with a drying detergent formulation and intensively mixed.
  • FR-A 2,160,661 and JP-A 60/37984 there are described processes for the production of enzyme granules by spraying a dispersed or dissolved enzyme (FR-A 2,160,661) or a powdered enzyme (JP-A 60/37984) onto a water-soluble or water-dispersible core material and fixing the enzymes on the core material by means of organic cohesive compounds or binders which are sprayed onto the core material before, simultaneously or after the enzymes have been applied to the core material.
  • the enzyme coated core materials such obtained are subsequently covered by a protective coating.
  • the present invention is a method for the production of dust free enzyme containing particles.
  • the method comprises the steps of:
  • a fluid bed dryer typically, such devices comprise a dryer consisting of a circular product chamber that has a porous grid on the bottom and is open on the top to be put up against a conical shaped expansion chamber of a larger diameter than the circular product chamber.
  • a dryer consisting of a circular product chamber that has a porous grid on the bottom and is open on the top to be put up against a conical shaped expansion chamber of a larger diameter than the circular product chamber.
  • the initial step in the method involves introducing a particulate, hydratable core material into the reaction chamber of the fluidized bed reactor and suspending the particles therein on a stream of air.
  • the core particles are of a highly hydratable material, i.e. a material which is readily dispersible or soluble in water.
  • the core material should either disperse (fall apart by failure to maintain its integrity) or solubilize by going into a true solution.
  • Clays bentonite, kaolin
  • non-pareils and agglomerated potato starch are considered dispersible.
  • Non-pareils are spherical particles consisting of a solid core that has been rounded into a spherical shape by binding layers of powder to the core in a rotating spherical container.
  • the non-pareils used in the examples which follow have a sugar (typically sucrose) crystal core less than 0,3 mm (-50 mesh on the U.S. Standard Sieve Series) that was rounded by binding layers of corn starch onto the core using sugar as a binder.
  • the sugar used for binding was dissolved in water (50% w/w) and sprayed onto a mixture of sugar and corn starch while they were being rotated in a 167,64 cm (66 inch) Groen Stainless Steel Rotating Pan which were then heated to drive off the water.
  • the crystals When the crystals had been rounded into approximately 0,85 mm to 0,25 mm (-20 mesh to 60 mesh) spheres, they were dried and sieved whereupon the >0,85 mm, ⁇ 0,25 mm(-20 mesh +60 mesh) fractions were put back into the rotating pan and heated. They were then coated with a layer (approximately 10% w/w) of dextrin from an aqueous solution (50% w/w) that was sprayed onto the spheres while heating to drive off the water. The finished product was again sieved to 0,85 mm to 0,25 mm (-20 mesh +60 mesh). Salt particles (NaCl crystals, NaCl rock salt, NaHCO3) are considered soluble.
  • core particles can be non-pareils of a salt crystal, starch and a sugar solution or a sugar crystal, starch and a sugar solution with or without a final coat of dextrin or a confectionary glaze.
  • agglomerated trisodium citrate pan crystallized NaCl flakes, bentonite granules and prills, bentonite/kaolin/diatomaceous earth disk pelletized granules and sodium citrate crystals.
  • the core particle is of a material which is not dissolved during the subsequent spraying process and is of a particle size of from 150 to 2,000 ⁇ m (100 mesh to 10 mesh on the U.S. Standard Sieve Series) in its longest dimension.
  • Enzymes suitable for use in this method are those which are soluble or dispersible in an aqueous media and from which the water can be removed to leave a residual layer of enzyme on the surface of the core material.
  • Suitable enzymes include, for example, proteases (bacterial, fungal, acid, neutral or alkaline), amylases (alpha and beta) and lipases whose water solutions or dispersions are prepared by dispersing or dissolving a precipitated enzyme cake in water using vigorous agitation.
  • the enzyme precipitate is dissolved or dispersed at a level of 15% to 30% solids (w/w) of which 100% down to 30% is enzyme with the remaining solids comprising, e.g., metallic salts, binders, plasticizers and fragrances.
  • the dispersion including any optional binders, metallic salts, stabilizers or fragrances must have a viscosity of 10 to 5,000 mPa ⁇ s at room temperature low enough to be pumped and atomized for effective spray coating.
  • the enzyme is applied to the surface of the core material by fluidizing the core particles in a flow of air whereupon a solution containing the enzyme and optionally other solids is then atomized and sprayed into the fluidized bed.
  • the atomized droplets contact the surface of the core particles leaving a film of the solids adhering to the surface of the particles when the water is evaporated.
  • the enzyme coated particles When sufficient enzyme is applied to the core particles to provide the desired enzyme activity, the enzyme coated particles, while still suspended in the reaction chamber of the fluidized bed reactor, are coated with a uniform layer of a water soluble or water dispersible, macro-molecular, film-forming coating agent. This is accomplished in a manner similar to that used for application of the enzyme coating.
  • Suitable film-forming agents include, for example, fatty acid esters, alkoxylated alcohols, polyvinyl alcohols, ethoxylated alkylphenols and more specifically, polyethylene glycols (MW 1,000 to 8,000), linear alcohol alkoxylates (MW 1,450 to 2,670), polyvinyl pyrrolidone (MW 26,000 to 33,000), polymeric nonylphenyl ethoxylates (MW 1,975 to 4,315) and dinonylphenyl ethoxylate (average MW 6,900).
  • the net result of the process is to provide an enzyme coated core particle having a continuous layer of the film-forming material on its surface wherein there is applied sufficient enzyme and film-forming material to provide a total dry weight gain of 25% to 55% based on the weight of the particulate core material to thereby provide the desired dust free enzyme containing particle.
  • the dust free enzyme particles of the present invention can be used wherever enzymes are needed in an aqueous system. Thus, they can be used as additives to detergent formulations, for removing gelatin coatings on photographic films to aid in silver recovery, in the digestion of wastes from food processing plants for nitrogen recovery, in denture cleansers for removing protein bound stains and as a processing aid in waste water treatment.
  • the method of practicing the invention is further illustrated by the following examples where all mesh sizes are on the U.S. Standard Sieve Series, and the dryer is a ®Uni-Glatt * laboratory model fluid bed dryer with variable air temperature and flow through the bed.
  • the device has a 15,24 cm (6 inch) Wurster insert which consists of a container 13,97 cm (5-1/2") diameter by 16,51 cm (6-1/2")height) for the core material that fits against the bottom of the device's expansion chamber.
  • the plate on the bottom of the Wurster has holes in it to distribute the air through the bed with the holes in the center being of a larger diameter than the rest of the holes in the plate.
  • a cylindrical hollow tube (7cm (2-3/4)inches diameter by 15,24 cm (6 inches) length) called a partition is suspended above these larger diameter holes creating a higher air flow up through the partition than up around the outside of the partition.
  • the air flow is adjusted based on the quantity and density of the core particles so that the particles flow up inside the partition into the expansion chamber then fall back down outside the partition into the area with less air flow while the bed is kept fluidizing and drying. This difference in air flow creates a circular upward and downward movement of the particles.
  • the spray nozzle is installed at the bottom of the partition pointed upwards. This arrangement keeps the atomized liquid co-current with the motion of the cores being coated and results in a smooth coating.
  • the speed of the circular flowing motion of the cores is adjustable by regulating the amount of air going through the partition and the amount of air going around the outside of the partition.
  • the droplet size of the atomized enzyme solution spray is adjusted by adjusting the liquid pumping rate and the air pressure for atomization. The process can be accelerated by using counter current downward spray without using the Wurster column.
  • "Uni-Glatt” is a trademark of Glatt Process Technology GmbH
  • the height of the Wurster insert partition is adjustable vertically and was adjusted from 0,64cm (1/4 inch) to 1,9 cm (3/4 inch) up from the bottom plate.
  • denser core materials up to 3/4 of the holes outside the partition were blocked off to provide a higher linear velocity for the air to lift the particles up through the inside of the partition and maintain a smooth circulation of material through the spraying area.
  • the total air flow was adjusted to get a good flow of cores through the partition and keep the bed outside the partition fluidized.
  • Inlet air temperature was adjusted up to a maximum of 75°C so that the outlet as well as particle temperatures were below 50°C. Typical outlet temperatures during the coating process were 25°C to 40°C.
  • the solids level of enzyme slurry sprayed in was 15% to 30% of the solution (w/w).
  • Feed rate varied from 5 ml/min. to 20 ml/min. When a more soluble core material was used, a lower initial feed rate was essential to coat a layer of enzymes on the core before the feed rate was increased.
  • Atomization air pressure ranged from 1.0 to 1.5 bar.
  • a typical dry weight gain of the core material after enzyme coating is 10% to 35% depending on the final activity desired.
  • the enzyme coated core was further coated with a macro-molecular, film-forming, water soluble or water dispersible coating agent to seal the enzyme from contact with the atmosphere or persons handling the particle. After application of the enzyme and protective coating, the total dry weight gain based on the weight of the core material after the dust free coating is 25% to 55%.
  • the core materials are either salt or non-pareils.
  • Salt is totally soluble and water clear when dissolved and is inexpensive as a core material. Being a solid crystal and not a multicompound structure, it is less subject to breaking up during the coating process and the enzyme slurry can be sprayed at a faster rate.
  • the salt particles being cubes make them more difficult to coat because there is a greater tendency for poor binding between the film and the core.
  • enzyme coated salt crystals are more subject to film loss due to attrition from the corners of cubes striking the flat surfaces of others. This problem can be partially alleviated by adding binders or plasticizers to the enzyme slurry.
  • Suitable materials include carboxymethyl cellulose, sodium alginate, collagen, polyethylene glycol and ethoxylated alkylphenols in an amount of from 1 to 10% (w/w) of the total solids in the slurry.
  • the flat surfaces provide larger areas of contact between particles which can cause agglomeration thereby inhibiting the flow characteristics of the coated salt particles.
  • the non-pareils are spherical, can readily be coated with a continuous film and have less area of contact among particles thereby limiting agglomeration. The final spherical product has better flow characteristics than the cubic salt based enzyme product.
  • nonpareil particles prepared by spraying a sugar solution onto sugar crystals which were coated with starch followed by a final coat of dextrin, less than 0,6 mm, but greater than 0,25mm (-30 +60 mesh)
  • DAPU Detergent Alkaline Protease Unit
  • the enzyme coated particles were further coated with a nonylphenol ethoxylate having an average -molecular weight of 4315 marketed under the trademark ®Iconol NP-100 (BASF-Wyandott Corp.) by spraying 120g of its aqueous solution onto the particles in the Uni-Glatt device.
  • the solution which was 50% w/w, contained 60 g of the Iconol NP-100 and was sprayed at a rate of 8 ml/minute.
  • Iconol NP is a nonionic chemical compound composed of a nonylphenol hydrophobe and a polyoxyethylene group hydrophile all in one molecule.
  • the material is represented by the structural formula: with X being approximately 100 in the NP-100 material.
  • coated particles were further cosmetically coated with 260 g of an aqueous solution containing 82 g (31.5% w/w) titanium dioxide and 27 g (10.4% w/w) Iconol NP-100 at the feed rate of 8 ml/minute.
  • the Uni-Glatt operating conditions were the same as in Example 1 except that the Wurster insert was 1,9 cm (3/4 inch) from the bottom plate and the inlet temperature was in the 70-74°C range.
  • One thousand grams of ⁇ 0,6mm >0,25mm (-30 +60 mesh) non-pareils (sugar crystals-sugar solution-starch-dextrin-glaze) was charged to the Uni-Glatt and fluidized.
  • An aqueous enzyme slurry with 19% (w/w) dry solid having activity of 643.8 DAPU/g and 252,632 MWU/g (modified Wohlgemuth unit per gram) was fed into the dryer for coating at the rate of 12 ml/min.
  • a total of 2000 g of enzyme slurry containing 380 g of enzyme solid was used.
  • the enzyme coated particles were further coated with 146 g of a 50% (w/w) solution containing 73 g of polyethylene glycol (MW 4000) in water at a feed rate of 12 ml/min. and an inlet air temperature of 50-54°C.
  • the enzyme coated salt crystals were further coated with 20.3 kg of a solution containing 6.1 kg (30% w/w) Iconol NP-100 in water at the feed rate of 125 ml/min. for 80 minutes, 167 ml/min. for 30 minutes, and 227 ml/min. for 22 minutes.
  • the GPCG-60 fluidized bed dryer is a production model fluid bed spray coater very similar in design to the Uni-Glatt except that it has a proportionally taller expansion chamber. It was operated under the following conditions:
  • the enzyme coated particles were further coated with 9.7 kg of a solution containing 2.91 kg (30% w/w) Iconol NP-100 in water at the flat feed rate of 36 ml/min. for 81 minutes.
  • the particles were further coated with 11.6 kg of an aqueous solution containing 3.48 kg TiO2 (30% w/w) and 1.39 Iconol NP-100 (12% w/w) at the feed rate of 50 to 55 ml/min. for 214 minutes.
  • the enzyme coated particles were further coated with 2.6 kg of an aqueous solution containing 50% (w/w) Iconol NP-100 and 50% water.
  • the solution was atomized at a spray rate of 70 g/min. at 50°C inlet temperature. Holding the inlet air at 50°C resulted in a product temperature of 37 to 41°C.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • Genetics & Genomics (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Biotechnology (AREA)
  • Molecular Biology (AREA)
  • Biochemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Microbiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Detergent Compositions (AREA)
  • Enzymes And Modification Thereof (AREA)
  • Immobilizing And Processing Of Enzymes And Microorganisms (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Medicinal Preparation (AREA)
EP86102374A 1985-03-05 1986-02-24 Dust free particulate enzyme formulation Expired - Lifetime EP0193829B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/708,584 US4689297A (en) 1985-03-05 1985-03-05 Dust free particulate enzyme formulation
US708584 1985-03-05

Publications (3)

Publication Number Publication Date
EP0193829A2 EP0193829A2 (en) 1986-09-10
EP0193829A3 EP0193829A3 (en) 1988-11-23
EP0193829B1 true EP0193829B1 (en) 1991-09-18

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Application Number Title Priority Date Filing Date
EP86102374A Expired - Lifetime EP0193829B1 (en) 1985-03-05 1986-02-24 Dust free particulate enzyme formulation

Country Status (9)

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US (1) US4689297A (da)
EP (1) EP0193829B1 (da)
JP (2) JPS61209589A (da)
BR (1) BR8600926A (da)
CA (1) CA1267622C (da)
DE (1) DE3681468D1 (da)
DK (1) DK175435B1 (da)
ES (1) ES8704203A1 (da)
MX (1) MX163251B (da)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7671005B2 (en) 2004-02-13 2010-03-02 The Procter & Gamble Company Active containing delivery particle

Families Citing this family (166)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5009994A (en) * 1986-03-24 1991-04-23 Em Diagnostic Systems, Inc. Particles containing mannitol suitable for tabletting into diagnostic reagents
US4820627A (en) * 1986-03-24 1989-04-11 Em Diagnostic Systems, Inc. Method of preparing particles suitable for tabletting into diagnostic reagents
EP0270608B1 (en) * 1986-05-21 1990-08-22 Novo Nordisk A/S Coated detergent enzymes
FR2627984B1 (fr) * 1988-03-03 1990-08-17 Sanofi Sa Composition pulverulente a base d'alginate pour empreintes dentaires
US5318714A (en) * 1988-03-14 1994-06-07 Novo Nordisk A/S Stabilized particulate composition
EP0404806B1 (en) * 1988-03-14 1992-03-11 Novo Nordisk A/S Stabilized particulate composition
US5733763A (en) * 1988-08-19 1998-03-31 Novo Nordisk A/S Enzyme granulate formed of an enzyme-containing core and an enzyme-containing shell
WO1991006638A1 (en) * 1989-10-31 1991-05-16 Genencor International, Inc. Dust-free coated enzyme formulation
US5814501A (en) * 1990-06-04 1998-09-29 Genencor International, Inc. Process for making dust-free enzyme-containing particles from an enzyme-containing fermentation broth
US5254283A (en) * 1991-01-17 1993-10-19 Genencor International, Inc. Isophthalic polymer coated particles
DE4119281A1 (de) * 1991-06-12 1992-12-17 Basf Ag Verfahren zur herstellung von enzymzubereitungen
EP0532777A1 (en) * 1991-09-18 1993-03-24 HAARMANN & REIMER CORP. Production of lysozyme containing particles
KR100278498B1 (ko) * 1991-10-07 2001-01-15 웨인 에이치. 피쳐 피복된 효소함유 과립
US5879920A (en) * 1991-10-07 1999-03-09 Genencor International, Inc. Coated enzyme-containing granule
US5324649A (en) * 1991-10-07 1994-06-28 Genencor International, Inc. Enzyme-containing granules coated with hydrolyzed polyvinyl alcohol or copolymer thereof
US5211985A (en) * 1991-10-09 1993-05-18 Ici Canada, Inc. Multi-stage process for continuous coating of fertilizer particles
JPH06511381A (ja) * 1991-10-10 1994-12-22 ジェネンコア　インターナショナル　インコーポレーテッド 無粉塵酵素の製造方法
US5256557A (en) * 1991-12-27 1993-10-26 Solvay Enzymes, Inc. Purified alkaline protease concentrate and method of preparation
CA2140530A1 (en) * 1993-05-18 1994-11-24 Carl S. M. Andela Process for dust-free enzyme manufacture
DE4322229A1 (de) * 1993-07-05 1995-01-12 Cognis Bio Umwelt Umhüllte Enzymzubereitung für Wasch- und Reinigungsmittel
IS1736B (is) * 1993-10-01 1999-12-30 Astra Ab Aðferð og tæki sem stuðla að aukinni samloðun agna
BE1008221A3 (fr) * 1994-03-28 1996-02-20 Anda Biolog Sa Support solide fixant au moins un composant a activite biologique comprenant un site reactionnel, stabilise et procede pour son obtention.
GB2291058B (en) * 1994-07-14 1998-12-23 Solvay Acid-stable and thermo-stable alpha-amylases derived from sufolobus species
JPH10508755A (ja) * 1994-11-18 1998-09-02 ジェネンコア インターナショナル インコーポレーテッド 被覆酵素顆粒
KR100413241B1 (ko) * 1995-05-29 2004-03-30 가오가부시끼가이샤 효소함유조립물및그제조방법
US6936289B2 (en) 1995-06-07 2005-08-30 Danisco A/S Method of improving the properties of a flour dough, a flour dough improving composition and improved food products
ATE268381T1 (de) * 1995-10-06 2004-06-15 Genencor Int Mikrogranulaten zur nahrungs- oder futteranwendung
WO1997039116A1 (en) * 1996-04-12 1997-10-23 Novo Nordisk A/S Enzyme-containing granules and process for the production thereof
US6248706B1 (en) * 1996-05-13 2001-06-19 Genencor International, Inc. Enzyme granulate for washing and cleaning
DE19619221A1 (de) * 1996-05-13 1997-11-20 Solvay Enzymes Gmbh & Co Kg Enzymgranulat für Wasch- und Reinigungsanwendungen
US5935889A (en) * 1996-10-04 1999-08-10 Abb Lummus Global Inc. Catalyst and method of preparation
US6383810B2 (en) 1997-02-14 2002-05-07 Invitrogen Corporation Dry powder cells and cell culture reagents and methods of production thereof
US6627426B2 (en) 1997-02-14 2003-09-30 Invitrogen Corporation Methods for reducing adventitious agents and toxins and cell culture reagents produced thereby
US20040022666A1 (en) * 1998-06-30 2004-02-05 Invitrogen Corporation Methods for reducing adventitious agents and toxins and cell culture reagents produced thereby
US20060003447A1 (en) * 2003-12-30 2006-01-05 Richard Fike Dry powder cells and cell culture reagents and methods of production thereof
ES2168236T3 (es) * 1997-04-09 2005-04-16 Danisco A/S Utilizacion de lipasa para mejorar las pastas de pan y los productos de panaderia.
EP0913468A3 (en) * 1997-07-22 2001-06-13 Dsm N.V. Bread improving comüposition
EP1021525A1 (en) * 1997-12-20 2000-07-26 Genencor International, Inc. Fluidized bed matrix granule
NZ505298A (en) * 1997-12-20 2002-10-25 Genencor Int Enzyme (protease) granule formulations with salt hydrate and polymer coating having high solubility and increased stability
CN1242060C (zh) 1997-12-20 2006-02-15 金克克国际有限公司 基体颗粒
US6156548A (en) * 1997-12-23 2000-12-05 Novo Nordisk A/S Immobilization of enzymes with a fluidized bed for use in an organic medium
US7144717B1 (en) 1998-03-24 2006-12-05 Genecor International, Inc. Oxidizing enzymes
EP1091765A4 (en) 1998-06-30 2001-10-24 Invitrogen Corp Methods for reducing adventitious agents and toxins and cell culture reagents produced thereby
US6268329B1 (en) 1998-06-30 2001-07-31 Nouozymes A/S Enzyme containing granule
ATE231186T1 (de) 1998-07-21 2003-02-15 Danisco Lebensmittel
ES2237209T3 (es) 1998-10-27 2005-07-16 Genencor International, Inc. Granulo de matriz.
MXPA01004750A (es) 1998-11-13 2005-07-01 Genencor Int Granulo de baja densidad de lecho fluidizado.
DE60026970T2 (de) 1999-01-08 2006-11-30 Genencor International, Inc., Palo Alto Zusammensetzungen mit niedriger dichte und partikeln der diese enthalten
PT1069832E (pt) * 1999-02-10 2004-08-31 Basf Ag Alimentacao para animais de um valor nutritivo mais elevado metodo para a sua producao e a sua utilizacao de um composto de polietileno glicol
DE19929257A1 (de) 1999-06-25 2000-12-28 Basf Ag Polymerbeschichtete, granulierte enzymhaltige Futtermittelzusätze und Verfahren zu deren Herstellung
CN100378218C (zh) * 1999-10-01 2008-04-02 诺沃奇梅兹有限公司 喷雾干燥的酶产品
JP2003514922A (ja) 1999-10-15 2003-04-22 ジェネンコア インターナショナル インコーポレーテッド 蛋白質含有顆粒および顆粒配合物
EP1239844B1 (en) 1999-12-20 2005-06-08 Nicholas J. Kerkhof Process for producing nanometer particles by fluid bed spray-drying
US8771740B2 (en) * 1999-12-20 2014-07-08 Nicholas J. Kerkhof Process for producing nanoparticles by spray drying
GB9930562D0 (en) * 1999-12-23 2000-02-16 Boc Group Plc Partial oxidation of hydrogen sulphide
EP1126017B1 (de) * 2000-02-18 2005-10-26 Glatt Ingenieurtechnik GmbH Verfahren zur Herstellung von Vollwaschmitteln und Vollwaschmittelkomponenten
EP1328612B1 (en) 2000-10-27 2007-04-25 Genencor International, Inc. Particle with substituted polyvinyl alcohol coating
JP2004521615A (ja) * 2000-11-06 2004-07-22 インヴィトロジェン コーポレーション 乾燥粉末細胞および細胞培養試薬およびその生産の方法
WO2002061427A1 (en) 2001-01-31 2002-08-08 Novozymes A/S Method of analysing granular composition by fluorescence analysis
US8076113B2 (en) 2001-04-02 2011-12-13 Danisco Us Inc. Method for producing granules with reduced dust potential comprising an antifoam agent
ATE449840T1 (de) 2001-05-15 2009-12-15 Novozymes As Alpha-amylasevariante mit veränderten eigenschaften
BR0209154A (pt) 2001-05-18 2004-07-20 Danisco Processo de preparação de uma massa com uma enzima
WO2003000625A2 (en) 2001-06-22 2003-01-03 Genencor International, Inc. Highly impact-resistant granules
ATE462781T1 (de) * 2001-11-30 2010-04-15 Life Technologies Corp Zellkulturmedien
WO2003059087A1 (en) * 2002-01-15 2003-07-24 Basf Ag Granulates containing feed-enzymes
US6887570B2 (en) * 2002-02-05 2005-05-03 Nestec Ltd. Coated clumping litter
US7429421B2 (en) * 2002-02-05 2008-09-30 Nestec, S.A. Coated clumping litter comprising non-swelling particles
EP1490485B1 (en) 2002-03-27 2015-03-04 Novozymes A/S Granules with filamentous coatings
EP2431048B1 (en) 2002-10-08 2015-03-11 Danisco US Inc. Phenolic binding peptides
CN101119795B (zh) 2002-10-09 2011-02-23 诺维信公司 一种改进粒子组合物的方法
US20040115304A1 (en) * 2002-12-16 2004-06-17 Frank Dubner Feesdstuffs additives containing L-lysine with improved abrasion resistance, and process for their production
ES2305576T3 (es) * 2002-12-24 2008-11-01 Genencor International, Inc. Granulos plastificados mecanicamente resistentes.
US7955814B2 (en) 2003-01-17 2011-06-07 Danisco A/S Method
US20050196766A1 (en) * 2003-12-24 2005-09-08 Soe Jorn B. Proteins
DE602004030000D1 (de) 2003-01-17 2010-12-23 Danisco Verfahren zur in-situ-herstellung eines emulgators in einem nahrungsmittel
CN1742084B (zh) 2003-01-27 2010-09-08 诺维信公司 颗粒的稳定化
EP1625208A4 (en) * 2003-05-12 2006-10-18 Genencor Int NEW LIPOLYTIC ENZYME LIP2
WO2004101760A2 (en) * 2003-05-12 2004-11-25 Genencor International, Inc. Novel lipolytic enzyme elip
US20100129862A1 (en) * 2003-05-12 2010-05-27 Jones Brian E Novel lipolytic Enzyme lip1
DE10360841A1 (de) * 2003-12-20 2005-07-14 Henkel Kgaa Helle, stabile, staub- und geruchsarme Enzymgranulate
US7718408B2 (en) * 2003-12-24 2010-05-18 Danisco A/S Method
WO2008090395A1 (en) 2007-01-25 2008-07-31 Danisco A/S Production of a lipid acyltransferase from transformed bacillus licheniformis cells
US7906307B2 (en) 2003-12-24 2011-03-15 Danisco A/S Variant lipid acyltransferases and methods of making
GB0716126D0 (en) 2007-08-17 2007-09-26 Danisco Process
GB0405637D0 (en) 2004-03-12 2004-04-21 Danisco Protein
CA2560613C (en) * 2004-03-22 2015-11-24 Solvay Pharmaceuticals Gmbh Oral pharmaceutical compositions of lipase-containing products, in particular of pancreatin, containing surfactants
CN101052702B (zh) 2004-07-16 2013-01-09 杜邦营养生物科学有限公司 脂肪分解酶及其在食品工业中的应用
DK2258209T3 (da) 2004-09-27 2015-08-31 Novozymes As Phytasegranuler i dyrefoder
US20060073193A1 (en) * 2004-09-27 2006-04-06 Novozymes A/S Enzyme granules
DE102005036346A1 (de) * 2005-07-29 2007-02-01 Henkel Kgaa Beschichtete Kern-Schale-Aggregate
US20100015588A1 (en) * 2005-07-20 2010-01-21 Satoru Funakoshi Multilayered model tooth for dental training
HUE031042T2 (en) 2005-07-29 2017-06-28 Abbott Laboratories Gmbh Methods for producing pancreatin powder with low viral content
US9198871B2 (en) * 2005-08-15 2015-12-01 Abbott Products Gmbh Delayed release pancreatin compositions
US11266607B2 (en) * 2005-08-15 2022-03-08 AbbVie Pharmaceuticals GmbH Process for the manufacture and use of pancreatin micropellet cores
EP2497374A3 (en) 2005-10-12 2013-11-27 Danisco US Inc. Stable, durable granules with active agents
WO2007098756A1 (en) 2006-03-02 2007-09-07 Novozymes A/S High capacity encapsulation process
US10072256B2 (en) * 2006-05-22 2018-09-11 Abbott Products Gmbh Process for separating and determining the viral load in a pancreatin sample
ES2577430T3 (es) 2006-08-07 2016-07-14 Novozymes A/S Gránulos de enzima para pienso para animales
CN101500430B (zh) 2006-08-07 2014-02-19 诺维信公司 用于动物饲料的酶团粒
RU2009130732A (ru) * 2007-01-12 2011-02-20 ДАНИСКО ЮЭс, ИНК., ДЖЕНЕНКОР ДИВИЖН (US) Улучшенный способ сушки распылением
DK2155867T3 (da) * 2007-05-10 2016-01-25 Danisco Us Inc Stabile enzymatiske systemer til generering af persyre
BRPI0820503A2 (pt) * 2007-11-05 2015-06-16 Danisco Us Inc Variantes da alfa amilase de bacillus licheniformis com termoestabilidade aumentada e/ou dependência de cálcio diminuída
US8206966B2 (en) * 2007-11-05 2012-06-26 Danisco Us Inc. Alpha-amylase variants with altered properties
KR20100088675A (ko) * 2007-11-05 2010-08-10 다니스코 유에스 인크. 변경된 특성을 지닌 바실러스 종 ｔｓ-23 알파-아밀라아제의 변이체
US20090130063A1 (en) * 2007-11-15 2009-05-21 Solvay Pharmaceuticals Gmbh Process for separating and determining the viral load in a pancreatin sample
JP2011508755A (ja) * 2008-01-03 2011-03-17 アボット プロダクツ ゲゼルシャフト ミット ベシュレンクテル ハフツング 精製微生物リパーゼの顆粒を有する医薬組成物ならびに消化器疾患を予防又は治療する方法
EP2085070A1 (en) * 2008-01-11 2009-08-05 Procter & Gamble International Operations SA. Cleaning and/or treatment compositions
AU2009212526A1 (en) 2008-02-04 2009-08-13 Danisco Us Inc. TS23 alpha-amylase variants with altered properties
US8066818B2 (en) 2008-02-08 2011-11-29 The Procter & Gamble Company Water-soluble pouch
MX346974B (es) 2008-02-14 2017-04-07 Danisco Us Inc Granulos pequeños que contienen enzimas.
US20090209447A1 (en) * 2008-02-15 2009-08-20 Michelle Meek Cleaning compositions
US10557108B2 (en) 2008-03-28 2020-02-11 Novozymes A/S Triggered release system
MX2010013113A (es) 2008-06-06 2010-12-21 Danisco Inc Variantes de alfa-amilasa geobacillus stearothermophilus con propiedades mejoradas.
WO2010036515A1 (en) 2008-09-25 2010-04-01 Danisco Us Inc. Alpha-amylase blends and methods for using said blends
US20100267304A1 (en) * 2008-11-14 2010-10-21 Gregory Fowler Polyurethane foam pad and methods of making and using same
AU2009314545B2 (en) 2008-11-17 2014-04-10 Nestec S.A. Animal litters
US20100125046A1 (en) * 2008-11-20 2010-05-20 Denome Frank William Cleaning products
EP2414515A2 (en) 2009-04-01 2012-02-08 Danisco US Inc. Cleaning system comprising an alpha-amylase and a protease
WO2011000924A1 (en) 2009-07-03 2011-01-06 Abbott Products Gmbh Spray-dried amylase, pharmaceutical preparations comprising the same and use
WO2011005730A1 (en) 2009-07-09 2011-01-13 The Procter & Gamble Company A catalytic laundry detergent composition comprising relatively low levels of water-soluble electrolyte
BR112012000531A2 (pt) 2009-07-09 2019-09-24 Procter & Gamble composição detergente para lavagem de roupas catalítica que compreende teores relativamente baixos de eletrólito solúvel em água
WO2011090980A1 (en) 2010-01-20 2011-07-28 Danisco Us Inc. Mold treatment
GB2477914B (en) 2010-02-12 2012-01-04 Univ Newcastle Compounds and methods for biofilm disruption and prevention
US8222197B2 (en) 2010-03-12 2012-07-17 The Procter & Gamble Company Liquid detergent compositions comprising pH tuneable amido-gellants, and processes for making
MX2012010572A (es) 2010-03-12 2012-10-09 Procter & Gamble Gelificante diamido para utilizar en composiciones de productos de consumo.
GB201106408D0 (en) 2011-04-15 2011-06-01 Revolymer Ltd Novel composite
GB201106409D0 (en) 2011-04-15 2011-06-01 Revolymer Ltd Novel composite
GB201106391D0 (en) 2011-04-15 2011-06-01 Reckitt & Colman Overseas Novel composite
EP2537918A1 (en) 2011-06-20 2012-12-26 The Procter & Gamble Company Consumer products with lipase comprising coated particles
US9434932B2 (en) 2011-06-30 2016-09-06 Novozymes A/S Alpha-amylase variants
BR112014013236A2 (pt) 2011-12-02 2017-06-13 Bp Corp North America Inc composições e métodos para liquefação de biomassa
DK3699271T3 (da) 2012-02-07 2024-12-09 Danisco Us Inc Granulat- og pelletsammensætninger, der omfatter phytase og phytinsyre, og fremgangsmåde til fremstilling deraf
WO2013119470A1 (en) 2012-02-07 2013-08-15 Danisco Us Inc. Glycosylation as a stabilizer for phytase
US20130284637A1 (en) 2012-04-30 2013-10-31 Danisco Us Inc. Unit-dose format perhydrolase systems
US20150140172A1 (en) 2012-06-20 2015-05-21 Danisco Us Inc. Sandwich granule
DK2874506T3 (da) 2012-07-18 2019-07-15 Danisco Us Inc Fremgangsmåde til fremstilling af enzymgranulater
US20140193872A1 (en) 2012-12-14 2014-07-10 Bo Ava Chen Process for the Conversion of Cellulosic Feedstock Materials
WO2014145768A2 (en) 2013-03-15 2014-09-18 Bp Corporation North America Inc. Use of non-fungal 5' utrs in filamentous fungi
EP2857486A1 (en) 2013-10-07 2015-04-08 WeylChem Switzerland AG Multi-compartment pouch comprising cleaning compositions, washing process and use for washing and cleaning of textiles and dishes
EP2857487A1 (en) 2013-10-07 2015-04-08 WeylChem Switzerland AG Multi-compartment pouch comprising cleaning compositions, washing process and use for washing and cleaning of textiles and dishes
EP2857485A1 (en) 2013-10-07 2015-04-08 WeylChem Switzerland AG Multi-compartment pouch comprising alkanolamine-free cleaning compositions, washing process and use for washing and cleaning of textiles and dishes
AR098006A1 (es) 2013-10-15 2016-04-27 Danisco Us Inc Gránulo de arcilla
DK3068879T3 (da) 2013-11-14 2020-03-16 Danisco Us Inc Stabile enzymer opnået ved glykeringsreduktion
KR20160099629A (ko) 2013-12-16 2016-08-22 이 아이 듀폰 디 네모아 앤드 캄파니 점도 조절제로서의 폴리 알파-1,3-글루칸 에테르의 사용
ES2835703T3 (es) 2013-12-18 2021-06-23 Nutrition & Biosciences Usa 4 Inc Eteres de poli alfa-1,3-glucano catiónicos
WO2015123323A1 (en) 2014-02-14 2015-08-20 E. I. Du Pont De Nemours And Company Poly-alpha-1,3-1,6-glucans for viscosity modification
EP3116914B8 (en) 2014-03-11 2021-04-21 E. I. du Pont de Nemours and Company Oxidized poly alpha-1,3-glucan as detergent builder
US9714403B2 (en) 2014-06-19 2017-07-25 E I Du Pont De Nemours And Company Compositions containing one or more poly alpha-1,3-glucan ether compounds
EP3158043B1 (en) 2014-06-19 2021-03-10 Nutrition & Biosciences USA 4, Inc. Compositions containing one or more poly alpha-1,3-glucan ether compounds
DK3270893T3 (da) 2015-03-19 2021-11-01 Danisco Us Inc Stabile granulater med lav indre vandaktivitet
CN107580606B (zh) 2015-04-03 2021-06-08 营养与生物科学美国4公司 凝胶化右旋糖酐醚
EP3374401B1 (en) 2015-11-13 2022-04-06 Nutrition & Biosciences USA 4, Inc. Glucan fiber compositions for use in laundry care and fabric care
WO2017083226A1 (en) 2015-11-13 2017-05-18 E. I. Du Pont De Nemours And Company Glucan fiber compositions for use in laundry care and fabric care
JP7045313B2 (ja) 2015-11-13 2022-03-31 ニュートリション・アンド・バイオサイエンシーズ・ユーエスエー・フォー，インコーポレイテッド 洗濯ケアおよび織物ケアにおいて使用するためのグルカン繊維組成物
WO2017091533A1 (en) 2015-11-26 2017-06-01 E. I. Du Pont De Nemours And Company Polypeptides capable of producing glucans having alpha-1,2 branches and use of the same
JP7105694B2 (ja) * 2015-12-30 2022-07-25 ライフ テクノロジーズ コーポレーション 層状の細胞培養粒子およびその製造方法
ES2920357T3 (es) 2017-11-10 2022-08-03 Nutrition & Biosciences Usa 4 Inc Polisacárido morfológico único
CN108277116B (zh) * 2018-02-11 2020-11-27 山西勇宁记科技有限公司 一种洗脸清洁皂用酵素颗粒及其制备方法与应用
CA3098454A1 (en) 2018-04-26 2019-10-31 Danisco Us Inc Method for increasing stability of phytase in a solid composition and a granule composition comprising phosphate and phytase
CN112469825A (zh) 2018-09-11 2021-03-09 诺维信公司 用于饲料组合物的稳定颗粒
BR112022000351A2 (pt) 2019-07-09 2022-05-10 Dupont Nutrition Biosci Aps Composições de enzima particuladas revestidas de gordura
AU2020375621A1 (en) 2019-10-28 2022-04-28 Danisco Us Inc Methods and compositions for remediating cyanuric acid in aqueous liquids
US20230364203A1 (en) 2020-10-07 2023-11-16 Novozymes A/S New Granules for Animal Feed
CN117957318A (zh) 2021-09-13 2024-04-30 丹尼斯科美国公司 含有生物活性物质的颗粒
DK202300049Y4 (da) 2023-03-31 2025-01-30 Dsm Ip Assets Bv Hidtil ukendt enzymsammensætning og hidtil ukendt ølbrygningsfremgangsmåde
EP4687490A1 (en) 2023-03-27 2026-02-11 DSM IP Assets B.V. Enzyme composition and beer brewing process

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6037984A (ja) * 1983-08-09 1985-02-27 Showa Denko Kk 酵素粒剤の製造法

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA888690A (en) * 1966-04-25 1971-12-21 B. Mccarty Charles Enzyme-containing detergent compositions
US3519570A (en) * 1966-04-25 1970-07-07 Procter & Gamble Enzyme - containing detergent compositions and a process for conglutination of enzymes and detergent compositions
US3650961A (en) * 1969-07-18 1972-03-21 Monsanto Co Process for preparing particulate products having preferentially internally concentrated core components
US4016040A (en) * 1969-12-10 1977-04-05 Colgate-Palmolive Company Preparation of enzyme-containing beads
GB1362365A (en) * 1970-07-28 1974-08-07 Novo Terapeutisk Labor As Production of enzyme preparations
GB1415301A (en) * 1971-11-18 1975-11-26 Unilever Ltd Enzyme-containing granule
GB1377725A (en) * 1972-02-18 1974-12-18 Procter & Gamble Method of encapsulating enzymes
GB1435905A (en) * 1972-11-03 1976-05-19 Unilever Ltd Enzyme granules
GB1483591A (en) * 1973-07-23 1977-08-24 Novo Industri As Process for coating water soluble or water dispersible particles by means of the fluid bed technique
US4087368A (en) * 1974-02-11 1978-05-02 Colgate-Palmolive Company Water-soluble enzyme granules
GB1603640A (en) * 1977-07-20 1981-11-25 Gist Brocades Nv Enzyme particles
DD151598A1 (de) * 1980-06-19 1981-10-28 Norbert Sieg Verfahren zur kontinuierlichen herstellung von wasch-und reinigungsmitteln
JPS6037983A (ja) * 1983-08-09 1985-02-27 Showa Denko Kk 酵素粒剤の製造方法
US4617272A (en) * 1984-04-25 1986-10-14 Economics Laboratory, Inc. Enzyme drying process

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6037984A (ja) * 1983-08-09 1985-02-27 Showa Denko Kk 酵素粒剤の製造法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7671005B2 (en) 2004-02-13 2010-03-02 The Procter & Gamble Company Active containing delivery particle

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DK175435B1 (da) 2004-10-18
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DK98186A (da) 1986-09-06
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US4689297A (en) 1987-08-25
JP2509073B2 (ja) 1996-06-19
JPH0662857A (ja) 1994-03-08
DK98186D0 (da) 1986-03-04
ES8704203A1 (es) 1987-03-16
JPH046351B2 (da) 1992-02-05
DE3681468D1 (de) 1991-10-24
CA1267622C (en) 1990-04-10
MX163251B (es) 1992-03-24
ES552640A0 (es) 1987-03-16
BR8600926A (pt) 1986-11-11

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